Grain size and concentrations of heavy metals (arsenic (As), cadmium (Cd), chromium (Cr), copper (Cu), mercury (Hg), lead (Pb), and zinc (Zn)) of 148 surface sediments and activities of ²¹⁰Pb and heavy metal concetrantions of one sediment core from the Pearl River Estuary were analyzed. The surface sediments were dominated by silt and sandy silt. Sediment type controlled the spatial distribution patterns of the heavy metals. The heavy metal concentrations in the sediments ranged from 3.34 to 37.11 mg/kg for As, 0.06 to 2.06 mg/kg for Cd, 12 to 130 mg/kg for Cr, 5.8 to 170.6 mg/kg for Cu, 0.01 to 0.25 mg/kg for Hg, 23 to 78 mg/kg for Pb, and 32 to 259 mg/kg for Zn. Both contents of clay and organic carbons were significantly positively correlated with heavy metals. The baseline values of elements in the study area were 12.97 mg/kg for As, 0.14 mg/kg for Cd, 68 mg/kg for Cr, 28.9 mg/kg for Cu, 0.08 mg/kg for Hg, 33 mg/kg for Pb, and 92 mg/kg for Zn. The metal enrichment factor (EF) and geoaccumulation index (Igeo) were calculated to assess anthropogenic contamination. Results showed slight to moderate Cd contamination in the region. Principle component analysis indicated that Cd could be attributed to anthropogenic sources; As and Hg were predominantly affected by human activities; and Pb, Cr, Cu, and Zn were associated with both natural and anthropogenic sources.